CN110441462A - The detection method of Chrysophanol in a kind of Chinese materia medica preparation and XUEMINGMU PIAN - Google Patents
The detection method of Chrysophanol in a kind of Chinese materia medica preparation and XUEMINGMU PIAN Download PDFInfo
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- CN110441462A CN110441462A CN201910693014.9A CN201910693014A CN110441462A CN 110441462 A CN110441462 A CN 110441462A CN 201910693014 A CN201910693014 A CN 201910693014A CN 110441462 A CN110441462 A CN 110441462A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The present invention relates to a kind of detection methods of Chrysophanol in Chinese materia medica preparation and XUEMINGMU PIAN.The preparation extracting method of test solution of the present invention is easier, directly, can be obviously shortened the preparation time of test sample；In conjunction with and free anthraquinone component all hydrolyzed, extract component is more complete；The preparation method of control medicinal material solution ensures the detection of Cassia obtusifolia L, subsequent to use preparation method identical with test solution, completely, adequately extracts anthraquinone component most of in medicinal material, improves subsequent detection accuracy；Using Chrysophanol as reference substance, Chrysophanol powder is directly prepared into reference substance solution, it is comparative strong, and accuracy is high, lamellae is silica gel g thin-layer plate, to guarantee that active principle to be detected is fixed on silica gel g thin-layer plate, and then to guarantee the accuracy of testing result effectively by test solution and control medicinal material solution and reference substance solution sample-adding on silica gel g thin-layer plate.
Description
One, technical field:
The present invention relates to Traditional Chinese medicine historical preparation technical fields, and in particular to Chrysophanol in a kind of Chinese materia medica preparation and XUEMINGMU PIAN
Detection method.
Two, background technique:
Chrysophanol is a kind of anthraquinone analog compound, has antibacterial action to various bacteria, can cough-relieving, the movement of promotion intestinal tube, rush
Make nervous excitation and muscular paralysis, also there is apparent inhibiting effect to murine melanoma, has occupied importantly in clinical pharmacy
Position.Chrysophanol as the detection project in drug examination criteria, determine with it is whether extremely heavy containing Chrysophanol in XUEMINGMU PIAN
It wants.
The thin-layer identification method of Chrysophanol in Semen Cassiae has been recorded at present are as follows:
This product 10 are taken, coating is removed, it is finely ground, add methanol 20ml, is ultrasonically treated 20 minutes, filtration, filtrate recycling design
To dry, residue adds water 10ml to make to dissolve, then plus hydrochloric acid 1ml, be heated to reflux 30 minutes, cool down immediately, extract 3 with ether shaking
Secondary, each 15ml merges ether extracted liquid, and low temperature recycles ether, and residue adds methanol 1ml to make to dissolve, as test solution.Separately
Depend on pine torch control medicinal material 0.5g, is made in the same way of control medicinal material solution.Chrysophanol reference substance is taken again, is added methanol that every 1ml is made and is contained
The solution of 0.5mg is tested as reference substance solution according to thin-layered chromatography (four general rules 0502 of Chinese Pharmacopoeia version in 2015), is inhaled
5 μ l of test solution, control medicinal material solution and each 1 μ l of reference substance solution are taken, is put respectively on same silica gel g thin-layer plate, with stone
The upper solution of oily ether (60~90 DEG C)-Ethyl formate-formic acid (15 ︰, 5 ︰ 1) is solvent, is unfolded, and takes out, dries, ultraviolet
It is inspected under light lamp (365nm).In sample chromatogram, on position corresponding with reference medicine chromatography, the fluorescence of same color is shown
Principal spot shows the fluorescence spot of same color at the position corresponding to the chromatogram of the reference substance.
But be only capable of proposing free anthraquinone component using existing detection method, it deducts a percentage point less, is unfavorable for greatly
The detection of yellow phenol cannot effectively control the quality of the pharmaceutical preparations.And extraction process is relatively complicated, and the time is longer.
Therefore, it is necessary to simplify the detection method of Chrysophanol, keep operating procedure simplicity, result accurate and reliable.
Three, summary of the invention
In view of this, the present invention provides a kind of detection method of Chrysophanol in Chinese materia medica preparation and XUEMINGMU PIAN, to rheum officinale
The Qualitive test of phenol has made optimal test sample and control medicinal material preparation method, has found suitable solvent, can be to this
Preparation carries out effective Qualitive test.
To achieve the above object, the technical solution adopted by the present invention are as follows:
The detection method of Chrysophanol in a kind of Chinese materia medica preparation and XUEMINGMU PIAN, it is characterised in that: the following steps are included:
1) test solution with XUEMINGMU PIAN is prepared；
Take with XUEMINGMU PIAN 10, remove coating, it is finely ground, add dilute hydrochloric acid 20ml and chloroform 30ml, it is small to be heated to reflux 1
When, it lets cool, divides and take chloroform liquid, hydrochloric acid solution uses chloroform 20ml shaking to extract again, merges chloroform extracting solution, recycling
Solvent is to doing, and residue adds methanol 1ml to make to dissolve, as test solution；
2) control medicinal material solution is prepared；
3) reference substance solution is prepared；
4) it is tested according to thin-layered chromatography (four general rules 0502 of Chinese Pharmacopoeia version in 2015), draws test solution, control
Medicinal material solution and reference substance solution are put respectively on same silica gel g thin-layer plate；
Using petroleum ether-Ethyl formate-formic acid upper solution as solvent, it is unfolded, takes out, dry；It sets under ultraviolet lamp
It inspects；
Compare the spot of the test sample and the spot of the control medicinal material and reference substance, in determining and XUEMINGMU PIAN whether
Contain cassia seed and Chrysophanol.
The method for preparing control medicinal material solution are as follows: depend on pine torch control medicinal material 0.5g, water 20ml is added to decoct 1 hour, filtration,
Filtrate adds hydrochloric acid 4ml and chloroform 30ml, is heated to reflux 1 hour, lets cool, and divides and takes chloroform liquid, hydrochloric acid solution uses trichlorine again
Methane 20ml shaking is extracted, and merges chloroform extracting solution, recycling design is to doing, and residue adds methanol 1ml to make to dissolve, as control
Medicinal material solution.
The method for preparing reference substance solution are as follows: take Chrysophanol reference substance, add methanol that solution of every 1ml containing 0.5mg is made, make
For reference substance solution.
In the step 4):
Test solution is 5 μ l, and control medicinal material solution is 3~5 μ l, reference substance solution is 1 μ l；
Petroleum ether-Ethyl formate-formic acid volume ratio is 15:5:1；Petroleum ether boiling range is 60~90 DEG C；
The wavelength of ultraviolet light is 365nm.
In the step 4: compare the spot of the test sample and the spot of the control medicinal material and reference substance, determine and
Whether contain cassia seed in XUEMINGMU PIAN and Chrysophanol includes:
In sample chromatogram, at the same position of control medicinal material spot, the test sample whether there is identical fluorescence
Principal spot, and if it exists, contain Cassia obtusifolia L in Chinese materia medica preparation to be detected；If it does not exist, it is not contained in Chinese materia medica preparation to be detected
Cassia obtusifolia L；
At the same position of reference substance spot, the test sample whether there is identical fluorescence spot, and if it exists, to be checked
It surveys in Chinese materia medica preparation and contains Chrysophanol；If it does not exist, Chrysophanol is not contained in Chinese materia medica preparation to be detected.
Compared with prior art, the invention has the advantages that and effect:
1, thin-layered chromatography identification Chrysophanol in the present invention, the preparation combination preparation extraction process of test solution, directly
Hydrolysis, extracting method is easier, directly, can be obviously shortened the preparation time of test sample；
2, in the present invention test solution preparation, in conjunction with and free anthraquinone component all hydrolyzed, be extracted into
Divide more completely, so that testing result is more accurate.
3, the present invention and the preparation variety Chrysophanol classics detection method of current edition Chinese Pharmacopoeia compare, thin-layer chromatography condition
Rationally, method is feasible, and map spot is more clear, and separating degree is more preferable, and specificity is strong, and reproducibility, durability are preferable.
Four, Detailed description of the invention:
Fig. 1 is to use now to record the thin layer identification figure that method detects Chrysophanol in Chinese materia medica preparation；
Fig. 2 is the thin layer identification figure detected using the method for the present invention to Chrysophanol in Chinese materia medica preparation；
Fig. 3 is the different lamellae investigation figures detected using the method for the present invention to Chrysophanol in Chinese materia medica preparation；
Fig. 4 is the different temperature and humidity investigation figures detected using the method for the present invention to Chrysophanol in Chinese materia medica preparation；
Fig. 5 is that the thin layer method detected using the method for the present invention to Chrysophanol in Chinese materia medica preparation verifies investigation figure；
In Fig. 1: 1,2 batches of samples of 2- and XUEMINGMU PIAN；3- cassia seed control medicinal material；4- Chrysophanol reference substance；
In Fig. 2: 1,3 batches of 2,3- and XUEMINGMU PIAN samples；4- cassia seed negative sample；5- Chrysophanol reference substance；6- Cassia
Sub- control medicinal material；
In Fig. 3: 1,3 batches of 2,3- and XUEMINGMU PIAN samples；4. cassia seed negative sample；5. Chrysophanol reference substance；6. Cassia
Sub- control medicinal material；
In Fig. 4: 1,3 batches of 2,3- and XUEMINGMU PIAN samples；4. cassia seed negative sample；5. Chrysophanol reference substance；6. Cassia
Sub- control medicinal material；
In Fig. 5: left figure: 1,3 batches of 2,3- and XUEMINGMU PIAN samples；4. Chrysophanol reference substance；5. cassia seed control medicinal material；
Right figure: 1,3 batches of 2,3- and XUEMINGMU PIAN 4. cassia seed negative sample of sample, 5. Chrysophanol reference substance, 6. cassia seeds pair
According to medicinal material.
Five, specific embodiment
It is limited below with reference to specific embodiment technical solution of the present invention is further:
Embodiment 1:
In order to improve the detection accuracy of Chrysophanol in Chinese materia medica preparation and XUEMINGMU PIAN, the present invention provides a kind of Chinese medicine systems
The detection method of Chrysophanol in agent, specifically includes the following steps:
The test sample of Chinese materia medica preparation to be detected is prepared, and test solution is made in the test sample, wherein in be detected
Medicine preparation is and XUEMINGMU PIAN that Chinese materia medica preparation to be detected is prepared into test sample, i.e., Chinese materia medica preparation to be detected is removed coat, ground
It grinds, is finely ground, powder is made, under the premise of meeting drug examination criteria, using conventional mortar, to above-mentioned Chinese medicine system to be detected
Agent is ground, and further, solution is made as test solution in the Chinese materia medica preparation to be detected after grinding；
Using cassia seed as control medicinal material, and control medicinal material solution is made in the cassia seed, specifically, depending on pine torch pair
According to medicinal material 0.5g, 20ml water is added, decoct 1 hour, decocting liquid is filtered, gained filtrate adds hydrochloric acid 4ml and chloroform
Control medicinal material solution is made according to the preparation method of test solution in 30ml；
Using Chrysophanol as reference substance, and reference substance solution is made in the reference substance, specifically, taking Chrysophanol conduct pair
According to product, above-mentioned Chrysophanol is Chrysophanol powder, can directly obtain, solution is made as reference substance solution in above-mentioned Chrysophanol；
5 μ l of test solution is drawn, 1 μ l of 3~5 μ l of control medicinal material solution and reference substance solution is put respectively in same silica G
On lamellae, specifically, by the test solution of above-mentioned requirements amount and control medicinal material solution and reference substance solution point Yu Tongyi
On silica gel g thin-layer plate, avoids and carry test solution and control medicinal material solution and right respectively using multiple silica gel g thin-layer plates
According to error brought by product solution, the accuracy to Chrysophanol detection is improved；
Using petroleum ether (60~90 DEG C)-Ethyl formate-formic acid (15:5:1) upper solution as solvent, to the silica gel
G lamellae is unfolded, is taken out, drying processing, and silica gel g thin-layer plate to be inspected is obtained；
It by the silica gel g thin-layer plate to be inspected, is inspected under 365nm ultraviolet lamp, so that the silica G thin layer to be inspected
The spot of the test sample and the spot of the control medicinal material and the reference substance are shown on plate；
Compare the spot of the test sample and the spot of the control medicinal material and the reference substance, determine it is described it is to be detected in
Whether contain Cassia obtusifolia L and Chrysophanol in medicine preparation.
In detection method provided by the invention, the test sample for preparing Chinese materia medica preparation to be detected, and by the test sample
Test solution is made, comprising steps of
The Chinese materia medica preparation to be detected 10 is taken, removes coating, and finely ground, it is accurately weighed, obtain Chinese materia medica preparation to be detected
Powder to be detected is placed in conical flask by powder；
In the Chinese materia medica preparation powder to be detected, add dilute hydrochloric acid 20ml and chloroform 30ml, be heated to reflux 1 hour,
It lets cool, divides and take chloroform liquid, the hydrochloric acid solution isolated；
It in the hydrochloric acid solution, then is shaken and is extracted with chloroform 20ml, divided and take chloroform liquid；
The chloroform liquid taken is divided to merge twice by described, recycling chloroform liquid obtains purifying substances, In to doing
1ml methanol is added in the purifying substances and dissolves the test sample, obtains test solution.
Using the preparation method of above-mentioned test solution, completely, adequately by rheum officinale in Chinese materia medica preparation and XUEMINGMU PIAN
Phenol adequately extracts, and using the method for direct hydrolysis, extracting method is easier, directly, can be obviously shortened the system of test sample
The standby time；The preparation of test solution in the present invention, in conjunction with and free anthraquinone component all hydrolyzed, extract component is more
Completely, in case the progress of subsequent detection work, improves detection accuracy.And it is molten that control medicinal material is made in the control medicinal material
Liquid, comprising steps of
Further, described using cassia seed as comparison medicine
Depend on pine torch control medicinal material 0.5g, 20ml water is added, decoct 1 hour, decocting liquid is filtered, the filter is obtained
Liquid；
By above-mentioned gained filtrate, add hydrochloric acid 4ml and chloroform 30ml, be heated to reflux 1 hour, let cool, divides and take three chloromethanes
Alkane liquid, the hydrochloric acid solution isolated；
It in the hydrochloric acid solution, then is shaken and is extracted with chloroform 20ml, divided and take chloroform liquid；
The chloroform liquid taken is divided to merge twice by described, recycling chloroform liquid obtains purifying substances, In to doing
1ml methanol is added in the purifying substances and dissolves the test sample, obtains control medicinal material solution.
Using the preparation method of above-mentioned control medicinal material solution, the water with Cassia obtusifolia L in Chinese materia medica preparation and XUEMINGMU PIAN is mentioned
Technique is identical, thus tentatively ensure the detection of Cassia obtusifolia L, it is subsequent using preparation method identical with test solution, and completely
, adequately anthraquinone component most of in Cassia obtusifolia L hydrolyzed, extract component is more complete, and it is quasi- to improve subsequent detection
True property.
Further, described using Chrysophanol as reference substance, and reference substance solution, including step is made in the reference substance
It is rapid: to take Chrysophanol powder as reference substance；Methanol is added in the reference substance, it is 0.5mg/ml that the reference substance content, which is made,
Reference substance solution.Chrysophanol powder is directly prepared into reference substance solution, it is comparative strong, and accuracy is high.
Further, the lamellae is silica gel g thin-layer plate effectively by test solution and control control medicinal material
Solution and reference substance solution sample-adding are on silica gel g thin-layer plate, to guarantee that active principle to be detected is fixed on silica gel g thin-layer plate
On, and then guarantee the accuracy of testing result.
Further, described that the test solution of respective corresponding amount and the control medicinal material solution and reference substance is molten
Liquid is put respectively on same silica gel g thin-layer plate, comprising: by the control medicinal material solution of test solution described in 5 μ l and 3~5 μ l
And 1 μ l reference substance solution, put on same silica gel g thin-layer plate respectively.
In the further solvent, petroleum ether (60~90 DEG C)-Ethyl formate-formic acid volume ratio is 15:5:1,
Upper solution is taken to be unfolded.
Further, silica gel g thin-layer plate to be detected described above, which is placed under 365nm ultraviolet lamp, inspects, provided by the invention
In Chinese materia medica preparation the detection method of Chrysophanol does not limit temperature and humidity, in the temperature and humidity of Laboratory Request
Under the conditions of, Chrysophanol can be detected using the detection method of Chrysophanol in Chinese materia medica preparation provided by the invention, please be join
See that Fig. 2, Fig. 2 are using the testing result figure provided by the invention for carrying out detection method to Chrysophanol in Chinese materia medica preparation, acceptance of the bid
Numbers 5 be the spot of Chrysophanol reference substance, and label 6 is the spot of cassia seed control medicinal material, and label 1-3 is the spot of 3 kinds of test samples,
Label 4 is the spot of cassia seed negative sample, is 24 DEG C in temperature, under conditions of relative humidity is 38%, obtains above-mentioned Fig. 2's
Testing result figure；Fig. 3 is referred to, Fig. 3 is the different thin layers detected using the method for the present invention to Chrysophanol in Chinese materia medica preparation
Plate investigates figure, and wherein label 5 is the spot of Chrysophanol reference substance, and label 6 is the spot of cassia seed control medicinal material, and label 1-3 is 3
The spot of kind test sample, label 4 is the spot of cassia seed negative sample, using Merck prefabricated board, obtains the inspection in left side in Fig. 3
Result figure is surveyed, using the testing result figure for from making sheet, obtaining right side in Fig. 3；Fig. 4 is referred to, Fig. 4 is using the method for the present invention pair
The different temperature and humidity investigation figures that Chrysophanol is detected in Chinese materia medica preparation, wherein label 5 is the spot of Chrysophanol reference substance, label
6 be the spot of cassia seed control medicinal material, and label 1-3 is the spot of 3 kinds of test samples, and label 4 is the spot of cassia seed negative sample,
It is 24 DEG C in temperature, under conditions of relative humidity is 38%, obtains the testing result figure in left side in Fig. 4, is 5 DEG C in temperature, phase
Under conditions of being 32% to humidity, the testing result figure in left side in Fig. 4 is obtained；Fig. 5 is referred to, Fig. 5 is using the method for the present invention
The thin layer method detected to Chrysophanol in Chinese materia medica preparation verifies investigation figure, and on the left of Fig. 5 in testing result figure, label 4 is big
The spot of yellow phenol reference substance, label 5 are the spot of cassia seed control medicinal material, and label 1-3 is the spot of 3 kinds of test samples, in temperature
It is 27 DEG C, under conditions of relative humidity is 22%, using the testing result figure for from making sheet, obtaining left side in Fig. 5, is examined on the right side of Fig. 5
It surveys in result figure, label 5 is the spot of Chrysophanol reference substance, and label 6 is the spot of cassia seed control medicinal material, and label 1-3 is 3 kinds
The spot of test sample, label 4 are the spot of cassia seed negative sample, are 21 DEG C in temperature, under conditions of relative humidity is 52%,
Using Merck prefabricated board, the testing result figure in left side in Fig. 5 is obtained；In the testing result figure that Fig. 3, Fig. 4, Fig. 5 are showed, supply
The spot and control medicinal material solvent of test sample solution and the spot of reference substance solution are shown clearly, so that quality inspection personnel can accurately be sentenced
Break with the presence or absence of cassia seed and Chrysophanol in Chinese materia medica preparation, to guarantee the quality of Chinese materia medica preparation and XUEMINGMU PIAN.
Comparative example:
The TLC method of existing cassia seed identifies: this product 10 taken, coating is removed, it is finely ground, and add methanol 20ml, is ultrasonically treated
20 minutes, filtration, for filtrate recycling design to dry, residue added water 10ml to make to dissolve, then plus hydrochloric acid 1ml, be heated to reflux 30 minutes, stand
It is i.e. cooling, it is extracted 3 times, each 15ml with ether shaking, merges ether extracted liquid, low temperature recycles ether, and residue adds methanol 1ml to make
Dissolution, as test solution.Separately depend on pine torch control medicinal material 0.5g, is made in the same way of control medicinal material solution.Chrysophanol pair is taken again
According to product, add methanol that solution of every 1ml containing 0.5mg is made, as reference substance solution, according to thin-layered chromatography (Chinese Pharmacopoeia 2015
Four general rules 0502 of version) test, draw 5 μ l of test solution, control medicinal material solution and each 1 μ l of reference substance solution, put respectively in
On same silica gel g thin-layer plate, using the upper solution of petroleum ether (60~90 DEG C)-Ethyl formate-formic acid (15 ︰, 5 ︰ 1) as solvent,
Expansion takes out, dries, inspect at ultraviolet lamp (365nm).In sample chromatogram, in position corresponding with reference medicine chromatography
It sets, shows the fluorescence principal spot of same color, at the position corresponding to the chromatogram of the reference substance, show the fluorescence spot of same color.
The Chrysophanol in Chinese materia medica preparation and XUEMINGMU PIAN is detected using prior art, testing result refers to
It is the spot of Chrysophanol reference substance marked as 4 in Fig. 1, Fig. 1, is the spot of cassia seed control medicinal material, label marked as 3
It is the spot of 2 kinds of test samples for 1-2, is 24 DEG C in temperature, relative humidity detects under conditions of being 52%, obtains above-mentioned Fig. 1
Testing result figure, testing result are as follows: in sample chromatogram, in position corresponding with cassia seed control medicinal material and reference substance chromatography
On, test sample shows the spot of essentially identical color in chromatography, but spot shows unobvious, influences sentencing for product quality
It is disconnected；Using detection method provided by the invention in Chinese materia medica preparation and XUEMINGMU PIAN cassia seed and Chrysophanol detect, examine
It surveys result referring to fig. 2, testing result: in sample chromatogram, on position corresponding with cassia seed reference medicine chromatography, shows identical
The fluorescence principal spot of color shows the fluorescence spot of same color on position corresponding with Chrysophanol reference substance chromatography, and spot is aobvious
Show aobvious, separating degree is good, clear rounding, and Chrysophanol has specificity for the identification of cassia seed, therefore select Chrysophanol to compare.
The testing result of more above two scheme finds that Chrysophanol thin-layer identification method detection spot provided by the invention is relative to existing
There is the detection method of technology to become apparent, after chromatographic apparatus analysis verifying, Chrysophanol thin layer provided by the invention identifies
Method condition is reasonable, and method is feasible, and specificity is strong, and reproducibility, durability are preferable.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the scope of the present invention, all
Changed using the equivalent structure that specification and accompanying drawing content of the invention are done, should be included in scope of patent protection of the invention
It is interior.
Claims (5)
1. the detection method of Chrysophanol in a kind of Chinese materia medica preparation and XUEMINGMU PIAN, it is characterised in that: the following steps are included:
1) test solution with XUEMINGMU PIAN is prepared；
Take with XUEMINGMU PIAN 10, remove coating, it is finely ground, add dilute hydrochloric acid 20ml and chloroform 30ml, be heated to reflux 1 hour,
It lets cool, divides and take chloroform liquid, hydrochloric acid solution uses chloroform 20ml shaking to extract again, merges chloroform extracting solution, recycles molten
Agent is to doing, and residue adds methanol 1ml to make to dissolve, as test solution；
2) control medicinal material solution is prepared；
3) reference substance solution is prepared；
4) it is tested according to thin-layered chromatography (four general rules 0502 of Chinese Pharmacopoeia version in 2015), draws test solution, control medicinal material
Solution and reference substance solution are put respectively on same silica gel g thin-layer plate；
Using petroleum ether-Ethyl formate-formic acid upper solution as solvent, it is unfolded, takes out, dry；It sets and is inspected under ultraviolet lamp；
The spot of the test sample and the spot of the control medicinal material and reference substance are compared, whether is contained in determining and XUEMINGMU PIAN
Cassia seed and Chrysophanol.
2. the detection method of Chrysophanol in a kind of Chinese materia medica preparation according to claim 1 and XUEMINGMU PIAN, it is characterised in that:
The method for preparing control medicinal material solution are as follows: depend on pine torch control medicinal material 0.5g, water 20ml is added to decoct 1 hour, filtration, filtrate
Add hydrochloric acid 4ml and chloroform 30ml, be heated to reflux 1 hour, let cool, divides and take chloroform liquid, hydrochloric acid solution uses chloroform again
20ml shaking is extracted, and merges chloroform extracting solution, recycling design is to doing, and residue adds methanol 1ml to make to dissolve, as control medicinal material
Solution.
3. the detection method of Chrysophanol, feature exist in a kind of Chinese materia medica preparation according to claim 1 or 2 and XUEMINGMU PIAN
In:
The method for preparing reference substance solution are as follows: take Chrysophanol reference substance, add methanol that solution of every 1ml containing 0.5mg is made, as right
According to product solution.
4. the detection method of Chrysophanol in a kind of Chinese materia medica preparation according to claim 3 and XUEMINGMU PIAN, it is characterised in that:
In the step 4):
Test solution is 5 μ l, and control medicinal material solution is 3~5 μ l, reference substance solution is 1 μ l；
Petroleum ether-Ethyl formate-formic acid volume ratio is 15:5:1；Petroleum ether boiling range is 60~90 DEG C；
The wavelength of ultraviolet light is 365nm.
5. the detection method of Chrysophanol in a kind of Chinese materia medica preparation according to claim 4 and XUEMINGMU PIAN, it is characterised in that:
In the step 4: comparing the spot of the test sample and the spot of the control medicinal material and reference substance, determining and blood is bright
Whether contain cassia seed in mesh piece and Chrysophanol includes:
In sample chromatogram, at the same position of control medicinal material spot, the test sample whether there is the main spot of identical fluorescence
Point, and if it exists, contain Cassia obtusifolia L in Chinese materia medica preparation to be detected；If it does not exist, Cassia is not contained in Chinese materia medica preparation to be detected
Sub- medicinal material；
At the same position of reference substance spot, the test sample whether there is identical fluorescence spot, and if it exists, in be detected
Contain Chrysophanol in medicine preparation；If it does not exist, Chrysophanol is not contained in Chinese materia medica preparation to be detected.
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